Synthesis,crystal structure and photophysical studies on a ruthenium(II) carbonyl hydrido compound based on 2,2′‐bipyridyl‐5,5′‐dicarboxylic acid (H2bpdc)

A novel complex, namely [Ru^II(PPh₃)(CO)(H)(Hbpdc)]·2MeOH ( 1 ) (H₂bpdc = 2,2′‐bipyridyl‐5,5′‐dicarboxylic acid), has been synthesized from the reaction of H₂bpdc with [Ru^II(PPh₃)₃(CO)(H)₂] in methanol under mild condition and characterized by elemental analysis, IR spectrum, ESI mass spectrometry, and single crystal X‐ray diffraction. The structure shows that the complex crystallizes in the monoclinic space group P2₁/c with unit cell parameters a = 11.8984(13) Å, b = 16.5180(18) Å, c = 25.5322(19) Å, β = 115.302(4)°, V = 4536.6(8) ų, Z = 4. This compound features a 1‐D supramolecular chain constructed via hydrogen bonds. Its photophysical properties have been investigated in MeOH solution and in the solid state at room temperature.     

Catenated molecular pattern in the crystal structure of a copper(II) complex with pyrazine-2,6-dicarboxylic acid and chloride ligands

The crystals of catena-dichloro-(dihydrogen pyrazine-2,6-dicarboxylato-O,O′,N,-N′) copper(II) dihydrate Cu[H₂(2,6-PZDC)]Cl₂?2H₂O are monclinic, space group C2/c with a = 11.658(2) Å, b = 6.778(1) Å, c = 16.390(3) Å, β = 98.90(3)^°, and Z = 4. Two adjacent copper(II) ions are bridged by a fully protonated pyrazine-2,6-dicarboxylic acid molecule which uses for bridging its O,O′,N-bonding moiety on one side and a single hetero-ring nitrogen atom on the other. Two chloride ions in axial position complete the octahedral coordination around the metal ions with bond distances: Cu–N 2.027(3) ÅA, Cu–N′ 2.005(3) ÅA, Cu–Cl. 2.281(1) ÅA, and Cu–O 2.446(2) ÅA. Copper(II) ions are located in the center of symmetry and are coplanar with the ligand acid molecule forming flat molecular chains propagating in the direction of the b axis. Hydrogen bonds via solvation water molecule link the chains into molecular layers parallel to the ac plane. Weak van der Waals type interactions operate between the layers.     

Synthesis, characterization and crystal structure of a mononuclear zinc(II) complex derived from 2-methoxy- 6-[(3-cyclohexylaminopropylimino)methyl]phenol

Colourless block-shaped crystals of Dichloro{2-methoxy-6-[(3-cyclohexylaminopropy-limino)methyl]phenolato}zinc(II) methanol, [Zn(C₁₇H₂₆N₂O₂)Cl₂].CH₃OH, have been obtained and characterized by elemental analysis, IR and X-ray single crystal determination. The complex crystallizes in the monoclinic space group P2₁/n with unit cell dimensions a=12.980(3) ?, b=13.139(3) ?, c=13.277(3) ?, β=107.00(3)°, V=2165.4(8) ?³, Z=4, R ₁=0.0631 and wR2=0.1110. X-ray structure determination revealed that the complex consists of a [Zn(C₁₇H₂₆N₂O)Cl₂] moiety and a lattice MeOH molecule. In the crystal structure, molecules are linked through intermolecular N–HO, C–HCl and O–HCl hydrogen bonds, forming chains. It is the first complex derived from the Schiff base ligand 2-methoxy-6-[(3-cyclohexylaminopropylimino)methyl]phenol.Supplementary materialCCDC-606067 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge at http://www.ccdccam.ac.uk/const/retrieving.html or from the Cambridge Crystallographic Data Centre (CCDC), 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44(0)1223-336033 or e-mail: deposit@ccdc.cam.ac.uk.     

Synthesis,crystal structure and spectral analysis of diaquatetrakis(N‐methylimidazole)Ni(II)(2,4,6‐tribromophenol)

Diaquatetrakis(N‐methylimidazole)Ni(II)(2,4,6‐tribromophenol), Ni(H₂O)₂(C₃N₂(CH₃))₄^.2(C₆H₃Br₃O), was synthesized via reaction of nickel sulphate and 2,4,6‐tribromophenolate in aqueous media in the presence of N‐methyl imidazole and sodium hydroxide. The complex crystalizes in the triclinic space group P1 with one formula unit of Ni(C₃H₃N₂(CH₃))₄(H₂O)₂.2(C₆H₃Br₃O) in the cell. The coordination around the Ni(II) ion is a slightly distorted octahedron, involving four N atoms from four different di(N‐methyl imidazole) ligand in the basal plane. The two oxygen atoms of the water molecules located at the apical positions result in an octahedral coordination. The two tribomophenol groups in the unit cell are connected via hydrogen‐bonds to the atoms of the coordination sphere, to build one dimensional chains along the a‐axis. For characterization of complex FTIR, UV spectroscopy, DSC and TGA thermal analysis were performed. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Different complexation behavior of a proton transfer compound obtained from 1,10‐phenanthroline and pyridine‐2,6‐dicarboxylic acid with Sn(IV), Sb(III) and Tl(I)

The different complexation methods of a proton transfer compound, (phenH)₂(pydc) (phen=1,10‐phenanthroline; pydcH₂= pyridine‐2,6‐dicarboxylic acid), are discussed and formation of [Sn(pydc)(phen)(OH)₂]·3H₂O ( 1 ), {[Sb(pydc)(phen)]₂O}·2DMSO·4H₂O( 2 ) and [(Tl(pydcH)]_n ( 3 ) complexes are reported. The characterization was performed using IR spectroscopy and X‐ray diffraction. The structures of Sn(IV) and Sb(III) complexes show that both cationic and anionic fragments of the starting proton transfer compound have been involved in the complexation. Whereas the structure of Tl(I) complex demonstrates that only the anionic fragment of (phenH)₂(pydc) is contributed to the complexation. The complexes 1‐3 show a variety of structural features including mononuclear, binuclear and polymeric structures. In compounds ( 1 ), ( 2 ) and ( 3 ) a large number of hydrogen bonds are observed. These interactions play an important role in the formation and stabilization of supramolecular systems in the crystal lattices. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal and Molecular Structure of Bis{2,6‐bis(hydroxymethyl)pyridine‐O,O,N}{μ‐bis(2‐hydroxymethylpyridyl)methanolate‐O,N}dicopper(II)di(propionate). First example of non‐coordinate propionate anoins

Bis{2,6‐bis (hydroxymethyl) pyridine‐O,O,N} {μ‐bis(2‐hydroxymethylpyridyl) methanolate‐O,N} dicopper(II) di(propionate) (CCDC 143763) has been prepared and studied by single‐crystal X‐ray diffraction methods at 293(2) K. The crystal structure consists of dimeric complex cation, [Cu₂(μ‐bhmp)₂(bhmpH)₂]⁺² and propionate anions (bhmp ‐ 2,6‐bis(hydroxymethyl) pyridine; bhmpH ‐ 2‐(6‐hydroxymethylpyridyl) methanolate ) and propionate anions. The complex cation contains two neutral and two monodeprotonated bhmp molecules, each coordinate to one Cu(II) atom in a tridentate chelating manner, via two O atoms and N atom. The monodeprotonated bmph molecules are also tridentate coordinate via N atom and only one O atom, which serve as bridge between two CuO₄N₂ moieties. The propionate anions are “ fixed” to the complex by the hydrogen bonds.     

Synthesis and crystal structure of Mn(II) and Zn(II) complexes with 1,3,5-tris(carboxymethoxyl)benzene ligand

Two complexes (H₂bipy)[M₂(TB)₂(H₂O)₈]·5H₂O (M = Mn 1, Zn 2) (bipy = 4,4′-bipyridine, H₃TB = 1,3,5-tris(carboxymethoxyl)benzene) were synthesized by the reaction of the corresponding metal salt with ligand H₃TB and 4,4′-bipy in an aqueous methanol solution at room temperature, respectively. Their structures were determined by single crystal X-ray diffraction analysis. Both complexes 1 and 2 crystallize in the triclinic space group with the crystal parameters of 1: a = 9.725(12) ?, b = 10.651(13) ?, c = 10.882(13) ?, α = 91.72(2)°, β = 96.41(2)°, γ = 97.72(2)°, V = 1109(2) ?³, Z = 1 and 2: a = 9.610(10) ?, b = 10.55(2) ?, c = 10.83(2) ?, α = 91.60(4)°, β = 95.32(2)°, γ = 97.73(4)°, V = 1082(3) ?³, Z = 1. Complexes 1 and 2 have the same dinuclear structure, in which each metal atom is six coordinated with distorted octahedral geometry by two oxygen atoms from two different TB³⁻ ligands and four ones from four coordinated water molecules. The dinuclear units are further linked by hydrogen bonding and π–π interactions to form the three-dimensional framework structure.     

Synthesis,characterization and crystal structure of a novel 2D Ni(II) complex with malate

An exploration of the nickel‐ malate‐bpa system under hydrothermal conditions, has led to the isolation of a novel framework {[Ni(Hmal)(bpa)]·2.5H₂O}_n ( 1 ) (Hmal = malate dianion, bpa = 1,2‐bi(4‐pyridyl)ethane). Single‐crystal X‐ray analyses reveal that it crystallizes in the orthorhombic space group Fdd2. a = 21.9944(13) Å, b =33.3369(19) Å, c = 10.3969(5) Å, β = 90°. The Ni^II ions are linked into an extended helical chain via Hmal molecules. Further these chains are united together through the bridging bpa to form a 2D grid layer, which exhibits a typical (6,3) topological network. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis,crystal structure and characterization of new transition metal compounds of bromophenols: Bis(2,4,6‐tribromophenolato) di(N‐methylimidazole)M(II) (M=Co,Cu)

Bis(2,4,6‐tribromophenolato)di(N‐methyl imidazole)M(II), where M stands for cobalt and copper metals, was synthesized via reaction of the corresponding metal sulphate and 2,4,6‐tribromophenolate in aqueous media in the presence of N‐methyl imidazole and sodium hydroxide. Although various crystallization procedures were applied only cobalt complex was obtained as single crystals. The Co(II) ion has a distorted octahedral enviroment involving two O atoms and two N atoms of the Bis(2,4,6‐tribromophenolato)di(N‐methyl imidazole) ligand. Powder x‐ray diffraction pattern of copper compound was used for cooper complex. For characterizations of complexes carbon, hydrogen and nitrogen elemental analysis, FTIR and UV spectroscopy, DSC thermal analysis and magnetic susceptibility measurements at room temperature were performed. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Spectroscopic and crystal structure analysis of diamminebis(2,4,6‐triiodophenolato‐O) copper(II)

The crystal structure of [Cu(C₆H₂I₃O)₂(NH₃)₂] (CCDC 238896) has been determined by x‐ray diffraction. This monomeric centrosymmetric Cu(II) complex crystallizes in the monoclinic system. The CuO₂N₂ coordination sphere is trans ‐planar, [Cu–O: 1.943(5) Å and Cu‐N: 1.972(7)] with the fifth and sixth coordination sites occupied by I atoms from the phenoxide ions [Cu–I₁: 3.3552(8) Å] to form a tetragonally elongated octahedral structure for CuO₂N₂I₂ coordination. The complex molecules hold together in a one dimensional chain true [100] direction by intermolecular hydrogen bonds. Differantial scanning calorimeter, FTIR and magnetic susceptibility measurements were also performed in order to identify the title complex. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and X‐ray structure of two conformational isomers of [Zn(medpt)(SCN)2], medpt = bis (3 – aminopropyl)methylamine

Two conformational isomers of [Zn (medpt)(NCS)₂], medpt=bis(3‐aminopropyl) methylamine, (1) and (2) have been synthesised and the crystal structures are determined using single crystal X‐ray diffraction. The structures of the complexes have been solved by Patterson method and refined by full‐matrix least‐ squares techniques to R1 = 0.0524 for (1) and R1 = 0.0506 for (2), respectively. The geometry around the Zn(II) centre in both isomers is distorted trigonal bipyramidal. The two pendent thiocyanate moieties in (1), with Zn–N–C angles 167.9(4)–173.9(4)º, coordinate the mental centre almost linearly while the corresponding coordinations in (2) are significantly bent [Zn–N–C angles 150.8(3)–153.1(2)°]. Intermolecular N–H…S hydrogen bonds stabilise the crystal packing in the complexes forming infinite chains parallel to the [100] direction. The combinations of molecular chains generate three/two dimensional supramolecular framework in complexes (1) and (2). (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and crystal structure of tetraiminediphenolate diiron(II) macrocyclic complex

The crystal structure of the binuclear tetraiminediphenolate diiron(II) macrocyclic complex [Fe₂(tidf)(CH₃OH)₄](ClO₄)₂ (tidf = tetraiminediphenolate ligand) is presented. The molecular structure (monoclinic, space group C2/c, Z = 4, a = 20.6903(14)Å, b = 11.0827(11) Å, c = 16.0494(15) Å, = 99.911(6) shows two iron(II) cores occupying distorted octahedral geometries with four methanol molecules bound axially. Main equatorial bond distances are 2.050(3) Å for Fe—O1 and 2.067(4) Å for Fe—N1 with a Fe Fe distance of 3.108(1) Å. Contrasting to the monoiron complex the macrocycle does not adopt a bent conformation being nearly coplanar with the maximum deviation from the least-squares plane of 0.18 Å.     

Synthesis,characterization and crystal structure of a novel Ni(II) coordination polymer with dipyrido[3,2‐a:2′,3′‐c]phenazine and 4,4′‐oxy(bisbenzoate)

A novel coordination polymer, [Ni(dppz)(oba)(H₂O)]·0.5H₂O (dppz = dipyrido[3,2‐a:2′,3′‐c]phenazine and oba = 4,4′‐oxy(bisbenzoate)) has been synthesized through hydrothermal method and characterized by IR, and single‐crystal X‐ray diffraction. It crystallizes in monoclinic, space group C2/c with a = 23.163(5), b = 18.211(4), c = 14.460(3) Å, α = γ = 90°, β = 100.45(3)°, V = 5998(2) ų, Z = 2. The structure was solved by direct methods and refined to R = 0.0866 (wR₂ = 0.1836). The compound exhibits interesting one‐dimensional chain structures, which are further stacked through π‐π interactions to form supramolecular double chains. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure analysis of {bis‐2,6‐(3,5‐dimethylprazolyl) pyridine‐dicyanato}copper(II)monohydrate

A mononuclear copper(II) complex, [Cu(dmpp)(OCN)₂(H₂O)], was synthesized using 2,6‐bis (3,5‐dimethylpyrazolyl) pyridine (dmpp) and cyanate anion (OCN), and characterized by single crystal X‐ray diffraction. The coordination around the Cu atom is a distorted square‐pyramid involving three N atoms from the dmpp ligand and one N atom from OCN at the basal plane. The O atom of the OCN group is located at the apical position. The Cu atom is located 0.2782(1) Å above the basal plane. The Cu atom is coordinated by different donor atoms of the OCN groups. The complex crystalizes in monoclinic space group P2₁/n, with unit cell dimensions a= 12.4413(12), b=11.1457(13), c=14.2203(12) Å, β=108.817(3)°, V= 1866.5(3) ų. The cell containes 4 molecules. In the crystal, there are three intermolcular and three intramolecular hydrogen bonds interactions. The Cu atom and crystal water O interactions is 5.574 Å. © 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim     

Synthesis,crystal structure,thermal behavior and luminescence property of a cobalt(II) complex of pyridine-2,6-dicarboxylic acid containing benzimidazole as auxiliary ligand

The new cobalt(II) complex [Co(pydca)(bim)₃] (1) (where H₂pydca = pyridine-2,6-dicarboxylic, bim = benzimidazole) has been synthesized and characterized by elemental analysis, Infrared spectroscopy, X-ray single crystal analysis, thermogravimetric and fluorescent analysis. Single crystal X-ray diffraction analysis reveals that the mononuclear complexes are linked by N–H…O hydrogen bonds. Fluorescent analysis reveals that complex 1 exhibits intense luminescence in ethanol solution at room temperature.     

Synthesis, characterization, and crystal structure of an iron(II) 5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane macrocyclic complex

The synthesis and detailed characterization of the macrocyclic complex [Fe(meso)(CH₃CN)₂](ClO₄)₂·2CH₃CN (meso: 5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane) based on analytical, spectrometric, spectroscopic and X-ray diffraction methods are reported herein. This is the first single crystal structure of an iron-meso complex ever reported in the literature. The molecular structure revealed a tetragonally distorted octahedral geometry with the iron(II) bound to four amine nitrogens in the equatorial plane, while the apical positions are occupied by acetonitrile molecules. The macrocycle adopts the most stable conformation with the six-membered rings in chair form, while the gauche conformation is seen for the five-membered rings. The compound crystallizes in the space group P2₁/n, with cell parameters a=10.139(1), b=12.237(1), c=13.311(1) ?, β=99.542(2)° and Z=2.Supplementary material CCDC-239983 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge at [or from the Cambridge Crystallographic Data Centre (CCDC), 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44(0)1223–336033; email: deposit@ccdc.cam.ac.uk].”     

Synthesis and crystal structure investigation of pyridine‐2‐(3′‐mercaptopropanoic acid)‐N ‐oxide

Pyridine‐2‐(3′‐mercaptopropanoic acid)‐N ‐oxide (I), is a higher homologue of 1‐oxopyridinium‐2‐thioacetic acid (II) [1]. It crystallizes in monoclinic space group P2₁ with a = 9.2168(2) Å, b = 4.1423(2) Å, c = 11.3904(4) Å, β = 98.65(2)°, V = 429.93(3) ų and Z = 2. The least‐squares refinement gave residual index R = 0.024 for 1070 observed reflections. The introduction of an additional methylene group in (II) causes a flip in the carboxylic acid group of (I) that facilitates the molecules to align infinite antiparallel chains through strong C–H···O interactions. The molecules are interlinked by O–H···O hydrogen bonding across the chains and forming an infinite screw chain along y‐direction. The molecular packing is stabilized by O–H···O and C–H···O hydrogen bonding and π‐π electron interactions. This is an important facet of the crystal packing. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

X-ray crystal structure of trans-bis(monoethanolamine) bis(saccharinato)nickel(II)

The crystal structure of trans-bis(monoethanolamine)bis(saccharinato)nickel(II), [Ni(C₇H₄NO₃S)₂(C₂H₇NO)₂], has been determined from X-ray diffraction data. The metal complex is monoclinic, with a = 11.0555(5), b = 8.9103(4), c = 11.3890(5) Å, = 105.0230(10)°, Z = 2, and space group P2_1/c . The structure consists of individual molecules. Two monoethanolamine molecules and two saccharinate anions coordinate the nickel atom forming a distorted octahedron. The monoethanolamine molecules act as a bidentate ligand and form five-membered trans chelate rings, which constitute the plane of the coordination octahedron, while two saccharinate ions behave as a monodentate ligand occupying the axial positions. Intermolecular hydrogen bonds link the molecules to form a three-dimensional infinite structure.     

Synthesis,characterization and crystal structure of bis{2-methoxy-6-[(2-diethylaminoethylimino)methyl]phenolato}thiocyanatocobalt(III) perchlorate

Brown block-shaped crystals of bis{2-methoxy-6-[(2-diethylaminoethylimino)methyl]phenolato}thiocyanatocobalt(III) perchlorate, the first cobalt(III) complex derived from the Schiff base ligand HL, [Co^III(L)(HL)(NCS)].ClO₄ (HL=2-methoxy-6-[(2-diethylaminoethylimino)methyl]phenol) have been obtained and characterized by elemental analysis and X-ray single crystal determination. The complex crystallizes in the monoclinic space group P2₁/c with unit cell dimensions a=16.087(3) ?, b=12.354(3) ?, c=16.762(3) ?, β=93.77(3)°, V=3324.1(12) ?³, Z=4, R ₁=0.0741 and wR2=0.1366. X-ray structure determination revealed that the complex consists of a [Co^III(L)(HL)(NCS)]⁺ cation and a disordered perchlorate anion. The Co atom in the cation is six-coordinate in an octahedral coordination. In the crystal structure, the perchlorate anions are linked to the cations through intermolecular C–H⋯O hydrogen bonds, forming zigzag chains running along the caxis. It is the first cobalt(III) complex derived from the Schiff base ligand HL.     

Synthesis and crystal structure of a cobalt(II) complex with tris(1-pyrazolylmethyl)amine

The synthesis of a cobalt(II) complex of tris(1-pyrazolylmethyl)amine (amtp) is reported. The complex [Co(amtp)Cl](BPh₄) crystallizes in the space group P-1, with a = 8.979(2), b = 19.329(3), c = 20.251(3) Å, = 93.321(2), = 93.685(3), = 98.930(2)°, and Z = 4. The Co(II) atom is nearly tetrahedrally coordinated by three pyrazole N-atoms and one Cl^–. The tertiary amine N-atom of amtp is only weakly coordinated to Co(II) atom at a Co—N(amine) distance of ca 2.40 Å.